Nitrite in environmental water samples is reduced at room temperature to nitric oxide in acidic medium containing vanadium (III). Nitrate is also rapidly reduced after heating to 80-90 degrees C. Nitric oxide is removed from the reaction solution by scrubbing with helium carrier gas and is detected by means of a chemiluminescence NOx analyzer. Nanogram detection limits are obtained. The method has the advantage of not requiring highly acidic solutions for nitrate reduction and has been applied to the analysis of a variety of environmental waters, sediment, plant materials, and human urine and blood serum.

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